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[高效液相色谱-荧光检测法测定葡萄酒中的氨基甲酸乙酯]

[Determination of ethyl carbamate in wine by HPLC-FLD].

作者信息

Chen Dawei, Yin Shuoyan, Gao Jie, Zhong Qiding, Xu Xiaoming, Miao Hong, Zhao Yunfeng

机构信息

China National Centre for Food Safety Risk Assessment/Key Laboratory of Food Safety Risk Assessment, 100021, China.

出版信息

Wei Sheng Yan Jiu. 2014 Jan;43(1):121-4.

PMID:24564124
Abstract

OBJECTIVE

To evaluate the method for determining ethyl carbamate (EC) in wine by HPLC-FLD.

METHODS

Samples were derived and determined by HPLC with a fluorescence detector. Using a Agilent TC-C18 (250 mm x 4.6 mm x 5 microm) column and a mixture of CH3CN-0.02 mol/L CH3COONa as mobile phase for gradient elution. The incidence light wavelength was 233 nm, emission wavelength was 600 nm. The fluorescence reaction time was 30 min. The contents were calculated with an external standard.

RESULTS

The linearity was good in the ranges of 10-500 microg/L for EC. The average recovery rates of EC was 93.7%-106.0%. The RSD was 1.4%-2.8%, and the limit of quantification was 15 microg/L. GC-MS and HPLC-FLD were compared to evaluate for determining EC content in wine.

CONCLUSION

The HPLC-FLD method was simple, accurate and suitable for the determination of EC in multitudinous wine.

摘要

目的

评估采用高效液相色谱-荧光检测法(HPLC-FLD)测定葡萄酒中氨基甲酸乙酯(EC)的方法。

方法

样品经衍生化处理后,采用带荧光检测器的高效液相色谱进行测定。使用安捷伦TC-C18(250 mm×4.6 mm×5μm)色谱柱,以乙腈-0.02 mol/L醋酸钠混合溶液作为流动相进行梯度洗脱。激发光波长为233 nm,发射波长为600 nm。荧光反应时间为30分钟。含量采用外标法计算。

结果

EC在10 - 500μg/L范围内线性良好。EC的平均回收率为93.7% - 106.0%。相对标准偏差为1.4% - 2.8%,定量限为15μg/L。比较了气相色谱-质谱联用仪(GC-MS)和高效液相色谱-荧光检测法(HPLC-FLD)用于评估葡萄酒中EC含量的情况。

结论

高效液相色谱-荧光检测法简单、准确,适用于多种葡萄酒中EC的测定。

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